CN110724857A - Aluminum-rich alloy for fracturing ball, preparation method of aluminum-rich alloy and control method of hydrogen production rate of aluminum-rich alloy for fracturing ball - Google Patents
Aluminum-rich alloy for fracturing ball, preparation method of aluminum-rich alloy and control method of hydrogen production rate of aluminum-rich alloy for fracturing ball Download PDFInfo
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Abstract
The invention belongs to the technical field of aluminum-based alloys, and particularly relates to an aluminum-rich alloy for a fracturing ball and a preparation method thereof, and a control method of the hydrogen production rate of the aluminum-rich alloy for the fracturing ball. The aluminum-rich alloy for the fracturing ball comprises the following components in percentage by mass: 1-10% of M element, 5-15% of gallium, indium and tin element, and the balance of aluminum; the M element is copper or magnesium; the mass ratio of the gallium element, the indium element and the tin element is 65: 22: 13. the aluminum-rich alloy has higher compressive strength and hardness, and the reaction rate of the alloy and water can be controlled by adjusting the content of the M element, so that the use requirement of the fracturing ball can be met.
Description
Technical Field
The invention belongs to the technical field of aluminum-based alloys, and particularly relates to an aluminum-rich alloy for a fracturing ball and a preparation method thereof, and a control method of the hydrogen production rate of the aluminum-rich alloy for the fracturing ball.
Background
For oil and gas reservoirs, fracture reformation technology is an effective way to improve production. At present, the fracturing of a multistage ball-throwing sliding sleeve is a vertical well layering and horizontal well staged yield-increasing transformation technology which is widely applied at present, and in the technology, a fracturing ball is a key factor for determining whether the fracturing is successful. In order to meet the requirements of the pitching sliding sleeve staged fracturing technology, the fracturing ball needs to have the following characteristics at the same time: (1) the sliding sleeve has enough compressive strength and hardness, and can be opened; (2) the fracturing fluid can be automatically decomposed in the liquid such as formation water and the like so as to avoid blocking a channel after the fracturing operation is finished.
Aluminum and its alloys are capable of reacting with water to produce hydrogen gas, which can be decomposed in water. Therefore, the aluminum alloy material can be used as a fracturing ball. However, the surface of the aluminum is easy to generate a compact oxidation film, so that the aluminum and water cannot react continuously. The existing research shows that the three elements of gallium, indium and tin can generate a phase which is a liquid phase at room temperature in the aluminum alloy, and the phase can prevent the oxidation of aluminum so as to enable the aluminum to continuously react with water. For example, the Chinese patent application with publication number CN109988944A provides an aluminum alloy for hydrogen production by hydrolysis, the aluminum alloy is Al-Ga-In-Sn-Zn quinary alloy, wherein Ga, In and Sn elements produce GaInSn In the alloy4The phase is beneficial to damaging an oxide film formed on the Al crystal grains and can improve the hydrogen production rate. The introduction of Zn can further produce hydrogen rate, but the alloy is embrittled, has low strength and hardness, and is not suitable for being used as a fracturing ball.
Disclosure of Invention
The invention aims to provide an aluminum-rich alloy for fracturing balls, which has high compressive strength and hardness.
The invention also aims to provide a preparation method of the aluminum-rich alloy for the fracturing ball.
The invention also aims to provide a method for controlling the hydrogen production rate of the aluminum-rich alloy for the fracturing ball, which regulates and controls the decomposition rate of the aluminum-rich alloy by controlling the hydrogen production rate.
In order to achieve the purpose, the invention adopts the technical scheme that:
an aluminum-rich alloy for fracturing balls comprises the following components in percentage by mass: 1-10% of M element, 5-15% of gallium, indium and tin element, and the balance of aluminum; the M element is copper or magnesium; the mass ratio of the gallium element, the indium element and the tin element is 65: 22: 13.
preferably, the aluminum-rich alloy for the fracturing ball consists of the following components in percentage by mass: 1-8% of M element, 6% of gallium, indium and tin element, and the balance of aluminum; the M element is copper or magnesium; the mass ratio of the gallium element, the indium element and the tin element is 65: 22: 13.
in the aluminum-rich alloy, the mass ratio of the three elements of gallium, indium and tin is controlled, so that the three elements of gallium, indium and tin can form GaInSn in the alloy3Or GaIn4Sn phase, thereby enabling the aluminum to continuously react with water. Meanwhile, the introduced M element (copper or magnesium) can be dissolved in aluminum crystal lattices on one hand and can form AlMg and Al with aluminum respectively3Mg2Or Al2The Cu phase can improve the compressive strength and hardness of the aluminum-rich alloy under the combined action of solid solution strengthening and precipitation strengthening.
The aluminum-rich alloy has high compressive strength and hardness, wherein the highest compressive strength can reach 460MPa, and the highest hardness can reach 1.75 GPa. The aluminum-rich alloy has high elastic modulus of about 80GPa, so that the aluminum-rich alloy is difficult to deform and has good stability, and the use requirement of the fracturing ball is met.
The aluminum-rich alloy for the fracturing ball can be prepared by adopting the existing alloy preparation method. Preferably, the preparation method adopted by the invention comprises the following steps: taking raw materials containing M element, gallium element, indium element, tin element and aluminum element according to the proportion, and then carrying out vacuum arc melting to obtain the alloy.
Preferably, before vacuum arc melting, vacuum is firstly pumped to absolute pressure not more than 1 x 10-3Pa, and then filling argon to 0.25-0.35 atm.
Preferably, the current during vacuum arc melting is 450-550A.
Further preferably, the prepared ingot is overturned and smelted for at least 3 times so as to ensure that elements in the sample are uniformly distributed.
The elements in the aluminum alloy prepared by the preparation method are distributed in the aluminum matrix, so that the performance of the aluminum-rich alloy is further improved. The preparation method has simple process, and can prepare the aluminum-rich alloy with various dimensions.
The method for controlling the hydrogen production rate of the aluminum-rich alloy for the fracturing ball adopts the technical scheme that:
the method for controlling the hydrogen production rate of the aluminum-rich alloy for the fracturing ball keeps the total mass percent of the gallium element, the indium element and the tin element unchanged, and controllably adjusts the hydrogen production rate of the aluminum-rich alloy for the fracturing ball by reducing or increasing the mass content of the M element within the range of 1-10% of the mass percent of the M element.
Because formation pressures are different in different formations, fracturing balls with different compressive capacities need to be used for different formations. This requires that the aluminum alloy have a range of compressive capacity to meet the demands of fracturing the ball. The compressive capacity of the aluminum alloy is related to the types and contents of the introduced alloy elements, and different types and contents cause the change of the compressive capacity. Therefore, when the pressure resistance of the aluminum alloy is adjusted by adjusting the alloy elements, the influence factors are complicated and the adjustment direction is not clear, and the performance of the adjusted aluminum alloy may not meet the expectation, so that the adjustment is uncontrollable. During the use process of the fracturing ball, certain requirements are also imposed on the decomposition rate of the fracturing ball. This requires that the reaction rate (i.e. hydrogen production rate) of the aluminum alloy when reacting with water can be controlled to ensure that the decomposition rate of the aluminum alloy when used as a fracturing ball material can be controlled. The kind and content of the alloying elements introduced into the aluminum alloy also affect the reaction of aluminum with water, and the effect is often irregular.
The invention determines the control method of the introduced alloy element, namely the type and the content of the M element, to the hydrogen production rate and the compressive strength of the aluminum alloy, so that the change of the hydrogen production rate and the compressive strength has a certain rule. And the hydrogen production rate and the compressive strength can be adjusted in a larger range, so that the use requirements of fracturing balls of different stratums can be met.
After the M element is introduced into the aluminum alloy, part of the M element is dissolved in aluminum crystal lattices and occupies some active positions of aluminum, so that the effective contact area of the aluminum and water is reduced; m element can form M-Sn or M-In phase with indium and tin element respectively to promote In and Sn segregation and cause low melting point GaInSn at crystal boundary3Or GaIn4The precipitation amount of the Sn phase is reduced, even the Sn phase is not precipitated, so that the reaction speed of the molten aluminum is obviously reduced; the M element also forms an M-Al phase with aluminum, such as: AlMg, Al3Mg2，Al2Cu and the like, and the formed compounds cover the surface of the aluminum, so that the diffusion of the aluminum is hindered, the aluminum cannot contact with water, the reaction speed of the aluminum water is reduced, and the hydrogen conversion rate is remarkably reduced. As the content of the M element is reduced, the GaInSn3Or GaIn4The amount of Sn phase increases and the amount of M-Al phase decreases; as the content of the M element increases, GaInSn3Or GaIn4The amount of Sn phase decreases and the amount of M-Al phase increases. Therefore, the reaction rate of the aluminum-rich alloy and water, namely the hydrogen production rate can be controllably adjusted by regulating and controlling the change of the content of the M element.
Preferably, the mass percent of the M element is adjusted within a range of 2-8%.
More preferably, the total mass percentage of the gallium element, the indium element and the tin element is 6%.
Drawings
FIG. 1 is a diagram of a testing apparatus for reaction between different aluminum-rich alloys and water in the experimental examples of the present invention, in which 1 is a constant temperature water bath apparatus, 2 is distilled water, 3 is a reaction vessel, 4 is a thermometer, 5 is a thermocouple, 6 is a sample stage, 7 is a measuring cylinder, 8 is a fixed calibration bottle, 9 is a rubber tube, 10 is a plastic beaker, 11 is an electronic balance, 12 is a computer, and 13 is a gas collecting apparatus;
FIG. 2 is a graph of hydrogen production versus time for aluminum-rich alloys of the present invention with different magnesium contents at different water temperatures, wherein (a) is a graph of water temperature at 50 ℃; (b) is a relation curve at the water temperature of 60 ℃, and (c) is a relation curve at the water temperature of 70 ℃;
FIG. 3 is a graph showing the relationship between the magnesium content and the hydrogen production rate of the aluminum-rich alloy of the present invention at different temperatures;
FIG. 4 is a graph showing the relationship between the magnesium content and the compressive strength of the aluminum-rich alloy of the present invention;
FIG. 5 is a graph of the relationship between the magnesium content and the elastic modulus of the aluminum-rich alloy of the present invention;
FIG. 6 is a graph showing the relationship between the magnesium content and the hardness of the aluminum-rich alloy of the present invention;
FIG. 7 is a graph of hydrogen production versus time for aluminum-rich alloys of the present invention with varying copper content at a water temperature of 50 ℃;
FIG. 8 is a graph of hydrogen production versus time for aluminum-rich alloys of the present invention with varying copper content at 70 deg.C water temperature.
Detailed Description
The invention is further described with reference to the following specific embodiments and the accompanying drawings.
First, embodiment of aluminum-rich alloy for fracturing ball
Examples 1 to 8 in the following examples are aluminum-rich alloys in which the M element is magnesium, and examples 9 to 13 are aluminum-rich alloys in which the M element is copper:
example 1
The aluminum-rich alloy for the fracturing ball comprises the following components in percentage by mass: 1% of magnesium, and 6% of total mass percent of gallium, indium and tin, wherein the mass ratio of gallium, indium and tin is 65: 22: 13, and the balance of aluminum.
Examples 2 to 7
The aluminum-rich alloy for fracturing balls in examples 2 to 7 has basically the same composition as that in example 1 except that: the mass percentage of magnesium in example 2 was 2%, the mass percentage of magnesium in example 3 was 3%, the mass percentage of magnesium in example 4 was 4%, the mass percentage of magnesium in example 5 was 6%, the mass percentage of magnesium in example 6 was 8%, and the mass percentage of magnesium in example 7 was 10%.
Example 8
The aluminum-rich alloy for the fracturing ball comprises the following components in percentage by mass: 1% of copper, and 6% of total mass percent of gallium, indium and tin, wherein the mass ratio of gallium, indium and tin is 65: 22: 13, and the balance of aluminum.
Examples 9 to 13
The compositions of the aluminum-rich alloys for fracturing balls in examples 9-13 are essentially the same as in example 8, except that: the mass percent of copper in example 9 was 2%, the mass percent of copper in example 10 was 3%, the mass percent of copper in example 11 was 4%, the mass percent of copper in example 12 was 6%, and the mass percent of copper in example 13 was 8%.
Second, example of preparation method of aluminum alloy for fracturing ball
Example 14
The embodiment is a preparation method of the aluminum-rich alloy for the fracturing ball in embodiment 1, and the preparation method comprises the following steps:
(1) according to the mass percent of each element, the raw materials of Al, Ga, In, Sn, Mg and Cu have the following purities: 99.7%, 99.99%, 99.9%, 99.99%, in a water-cooled copper crucible of a non-consumable vacuum arc melting furnace (Shenyang Corp Ltd.);
(2) vacuumizing the smelting furnace to 1 x 10-3Pa or so, and then filling high-purity argon gas of about 0.3 atm; under the protection of argon, adopting 500A of smelting current to obtain an ingot; and (3) overturning and smelting the obtained cast ingot for 3 times, applying magnetic stirring, and then cooling to obtain the aluminum alloy.
The aluminum-rich alloys for fracturing balls in examples 2 to 13 were prepared by the preparation method in example 14. The prepared aluminum-rich alloy is processed by a machine tool to obtain the fracturing ball meeting the size requirement.
Comparative example 1
The aluminum-rich alloy of the comparative example is an Al-Ga-In-Sn alloy, and consists of the following components In percentage by mass: the total mass percentage of the gallium element, the indium element and the tin element is 6%, wherein the mass ratio of the gallium element to the indium element to the tin element is 65: 22: 13, and the balance of aluminum.
Third, a specific mode of a method for controlling the hydrogen production rate of the aluminum-rich alloy for fracturing balls is described in the following test examples.
Fourth, test example section
Test example 1: hydrogen production test and compressive strength test of magnesium-containing aluminum-rich alloy in examples 1 to 8
In this test example, the magnesium-containing aluminum-rich alloys of examples 1 to 8 were reacted with water at different temperatures, and the reaction time and the amount of hydrogen generated were measured by a water discharge method during the reaction. The schematic of the experimental set-up used in the test is shown in FIG. 1: a250 mL closed reaction vessel 3 was filled with 200mL of distilled water 2, and was placed in an HH-2 thermostatic waterbath apparatus 1 to maintain the temperature of the water set in the experiment, a thermometer 4 was placed in the HH-2 thermostatic waterbath apparatus 1 to observe the temperature of the water bath, and a thermocouple 5 was inserted into the closed reaction vessel 3 to measure the temperature of the distilled water 2, and the water level in a fixed calibration flask 8 was kept equal to the water level in a graduated cylinder 7 before the start of the reaction. When the water temperature reaches the set temperature, a sample (about 0.3g) on the sample table 6 is put into water, hydrogen generated in the reaction process enters the measuring cylinder 7 through the gas collecting device 13 and the rubber tube 9, the pressure in the measuring cylinder 7 is increased, so that the water in the measuring cylinder 7 enters the fixed calibration bottle 8 through the rubber tube 9, then the water level in the fixed calibration bottle 8 rises and flows into the plastic beaker 10 through the rubber tube 9, and the mass of the discharged water is recorded in the computer 12 through the JD1000-2 type electronic balance 11. The reaction temperature is controlled at 20 ℃ and the humidity is below 20%.
The specific test results are shown in fig. 2 and 3. In fig. 2, (a) is a graph of the amount of hydrogen reacted with water by the aluminum-rich alloy at a water temperature of 50 ℃, and (b) is a graph of the amount of hydrogen reacted with water by the aluminum-rich alloy at a water temperature of 60 ℃, and (c) is a graph of the amount of hydrogen reacted with water by the aluminum-rich alloy at a water temperature of 70 ℃, and (c) is a graph of time. FIG. 3 is a graph showing the relationship between the magnesium content in the aluminum-rich alloy and the hydrogen production rate at different temperatures.
As can be seen from fig. 2 and 3: when the mass percent of magnesium in the aluminum-rich alloy is 1-8%, the aluminum-rich alloy has high hydrogen production, 1000-1500 mL of hydrogen can be produced per gram of aluminum, and the change of water temperature and magnesium content has little influence on the total hydrogen production. For different water temperatures, the hydrogen production rate is reduced along with the increase of the content of magnesium in the aluminum-rich alloy, and the magnesium content and the hydrogen production rate show a linear relationship with a negative correlation. When the mass percent of magnesium in the aluminum-rich alloy is 10%, the hydrogen production rate of the aluminum-rich alloy is sharply reduced.
The compressive strength test of the aluminum-rich alloy in the embodiment 2 and the embodiments 4 to 7 is respectively carried out, and the specific test process is as follows: the compression test of the sample is carried out at room temperature by using a Gleeble 3800 universal tester, and the strain rate is 0.01s-1The sample size was 10mm × 10mm × 12 mm. The test results are shown in fig. 4. As can be seen from FIG. 4, the aluminum-rich alloy of the present invention has high compressive strength, all of which are above 250 MPa; and along with the increase of the magnesium content in the aluminum-rich alloy, the compressive strength of the aluminum-rich alloy is improved and can reach 460MPa at most. And the change of the compressive strength is large within the range of 2-8% by mass of magnesium.
The aluminum-rich alloys of examples 1 to 7 were tested for elastic modulus and hardness, respectively. The specific test method comprises the following steps: the hardness and elastic modulus of the test specimens were measured using a Nano 200 Nano indenter manufactured in the United states. The indenter used in the test was a Berkovich type triangular pyramid indenter with an indentation depth of 1 μm. Each test was tested for 10 impressions, the average of which was taken as the final result of the test specimen. The load-displacement data at final unloading were analyzed by the Oliver method and the Pharr method to determine hardness and modulus of elasticity.
The test results are shown in fig. 5 and 6. From the test results, it can be seen that the Mg content has little influence on the elastic modulus of the alloy, and the value is 80 +/-2 GPa. However, the Mg content is significant for the hardness of the alloy, and the hardness of the alloy gradually increases as the Mg content increases. When the content of the added Mg is 10 percent, the hardness value can reach 1.86 GPa.
Test example 2: hydrogen production test of copper-containing aluminum-rich alloys of examples 9 to 13
In this test example, the amounts of hydrogen generated by the reaction of the copper-containing aluminum-rich alloys of examples 9 to 13 and the aluminum-rich alloy of comparative example 1 with water at different temperatures were measured with reference to the test method of test example 1. Specific test results are shown in fig. 7 and 8. Fig. 7 shows hydrogen production amounts of Cu-rich aluminum alloys having different contents at a water temperature of 50 ℃, and fig. 8 shows hydrogen production amounts of Cu-rich aluminum alloys having different contents at a water temperature of 70 ℃.
The test result shows that the hydrogen production rate and the hydrogen conversion rate of the alloy are obviously reduced due to the addition of Cu, and the reduction trend is more obvious along with the increase of the addition amount of Cu in the alloy. For example, the hydrogen production rate is 152 mL/min-gAl and the hydrogen conversion rate is as high as 90% for the Al-Ga-In-Sn alloy without Cu at the water temperature of 50 ℃. When a small amount of Cu (1 wt.%) was added to the alloy, the hydrogen production rate was reduced to 135 mL/min. gAl, and the hydrogen conversion rate was 82.9%. As the Cu content increased to 3 wt.%, the hydrogen production rate and hydrogen conversion decreased still further, only 115mL/min · gAl and 32.5%. And continuously increasing the Cu content in the alloy to 8 wt.%, and reducing the hydrogen production rate and the hydrogen conversion rate of the alloy to 104 mL/min-gAl and 16.6%. However, as the water temperature increases, the reaction rate of the aluminum water reaction and the hydrogen conversion rate gradually increase.
The mechanical property test of the copper-containing aluminum-rich alloy shows that compared with the aluminum-rich alloy in the comparative example 1, the copper-containing alloy of the invention has better mechanical property.
From the test results of test examples 1 and 2, the aluminum-rich alloy of the present invention has the influence on both the hydrogen production rate and the mechanical properties due to the introduction of the element M. Along with the increase of the content of the M element in the aluminum-rich alloy, the hydrogen production rate is gradually reduced, and the mechanical property is improved. Therefore, when the aluminum-rich alloy is used as a fracturing ball, the fracturing ball can meet the use requirement by adjusting the content of the M element in the fracturing ball.
Claims (9)
1. The aluminum-rich alloy for the fracturing ball is characterized by comprising the following components in percentage by mass: 1-10% of M element, 5-15% of gallium element, indium element and tin element, and the balance of aluminum; the M element is copper or magnesium; the mass ratio of the gallium element, the indium element and the tin element is 65: 22: 13.
2. the aluminum-rich alloy for the fracturing ball as claimed in claim 1, which is composed of the following components in percentage by mass: 1-8% of M element, 6% of gallium element, indium element and tin element, and the balance of aluminum; the M element is copper or magnesium; the mass ratio of the gallium element, the indium element and the tin element is 65: 22: 13.
3. the preparation method of the aluminum-rich alloy for the fracturing balls as claimed in claim 1 or 2, which comprises the following steps: taking raw materials containing M element, gallium element, indium element, tin element and aluminum element according to the proportion, and then carrying out vacuum arc melting to obtain the alloy.
4. The method for preparing the aluminum-rich alloy for the fracturing ball as claimed in claim 3, wherein before the vacuum arc melting, the vacuum is firstly pumped to the absolute pressure of not more than 1 x 10-3Pa, and then filling argon to 0.25-0.35 atm.
5. The preparation method of the aluminum-rich alloy for the fracturing ball as claimed in claim 3, wherein the current used in the vacuum arc melting is 450-550A.
6. The method for preparing the aluminum-rich alloy for the fracturing ball as claimed in claim 3, wherein the prepared ingot is overturned to be melted at least 3 times.
7. The method for controlling the hydrogen production rate of the aluminum-rich alloy for the fracturing balls as claimed in claim 1 or 2, wherein the total mass percent of the gallium element, the indium element and the tin element is kept unchanged, and the hydrogen production rate of the aluminum-rich alloy for the fracturing balls is controllably adjusted by reducing or increasing the mass content of the M element within the range of 1-10% of the mass percent of the M element.
8. The method for controlling the hydrogen production rate of the aluminum-rich alloy for the fracturing balls as claimed in claim 7, wherein the mass percent of the M element is adjusted within a range of 2-8%.
9. The method for controlling the hydrogen production rate of the aluminum-rich alloy for fracturing balls as recited in claim 7 or 8, wherein the total mass percentage of the gallium element, the indium element and the tin element is 6%.
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| CN115637357B (en) * | 2021-07-20 | 2024-04-30 | 中国石油天然气股份有限公司 | Soluble aluminum alloy |
| CN117110106A (en) * | 2023-10-23 | 2023-11-24 | 中铝材料应用研究院有限公司 | Method for testing fatigue performance of aluminum alloy material in simulated high-pressure hydrogen environment |
| CN117110106B (en) * | 2023-10-23 | 2023-12-19 | 中铝材料应用研究院有限公司 | Method for testing fatigue performance of aluminum alloy material in simulated high-pressure hydrogen environment |
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